Product for printing textile yarns and fabrics



- 50 smooth printing paste giving excellent results.

Patented Apr. 9, 1940 PRODUCT FOR PRINTING TEXTILE YARNS AND FABRICS Moses L. Crossley, Plainfield, Roy H. Kienle and Chester A. Amick, Bound Brook, N. J., assignors, by mesne assignments, to American Cyanamid Company, New York, N. Y., a corporation of Maine No Drawing. Application August 11, 1938, Serial No. 224,258

12 Claims. (Cl. 8-70) This invention relates to a composition for considered as including certain essential comprinting textile fabrics and yarns. ponents to which other components may be added In ordinary printing processes, the printer buys if desired. The essential components are the separately the dyestufi, reducing agent, thickencolor itself, alkali, (usually alkali carbonates), re-

5 ing agent, assistants and the like, and prepares dueing agent (normally sulfoxylate) and his own printing paste therefrom. This involves Printing assistants, Wetting e t d the like a number of operations by the printer and the y also be P e t a d e included in more printing pastes prepared do not keep Very well so specific aspects of the present invention. It is that they are usually made up only in suflicient an important advantage that any of the well quantities for the immediate printing required. known printing assistants may be incorporated in The object of the present invention is t p the product of the present invention without in duce a dry product containing all of the ingrediny way reducing t effectiveness of he pro ents, that is to say, color, reducing agent, alkali, not and such P y y modifying agents as gum, assistants and the like, which product can y ne a the like y also be included- 15 be in the form of a powder, flakes, pellets or The present invention is not limited to any rains and requires only the addition of water or particular at C0101 in fact, to a Vat aqueous media to prepare a printing paste. since it is clearly applicable to the printing with It has been proposed in the past to mix a, vat stabilized diazo compounds admixed with coudye with Monopole soap and caustic alkali and D n components- The u used are the yp zo'then to dry the product and blend it dry with cal gums employed in printing such as British hydrosulfite. The product thus obtained was used gum, dextr t acanth, S a and the like, and

for vat dyeing. If, instead, it is attempted to obit is an advantage of the Present invention that tain a product for vat printing, although British the ordin y p g Practices in this respect are gum as well as vat dye, Monopole soap and causin no sense chan ed- 25 tic alkali are initially mixed together and subsee admixture o t e Wet ingredients y be quently dry blended with a reducing agent, e. g., effected in any suitable manner which will prosulfoxylate, the product will not form a satisfacduce a complete homogeneous mixture. y tory paste and very inferior prints result. satisfactory results are obtained by mixing as a According to the present invention, all of the rather thick paste, for example in a dough mixer,

30 ingredients are mixed wet and the product then and although the invention is in no sense limited dried and suitably comminuted. When the dryo this Particular method of admixture, in a more ing is effected carefully so as not to overheat, specific aspect this preferred modification is inthe dry product may be -formed into a printing eluded. paste by the simple addition of water or suitable e drying of the homogeneously admixed 5 aqueous media and excellent prints are obtained components is very important. In general, this being equal and in some cases slighly superior to should be effected at a temperature below that prints made in the ordinary way; that is to say, at which the hydratable constituents such as the where all of the ingredients are formed into a gum are afiected to the extent that they do 'not paste without passing through a stage of dry readily rehydrate. Preferably, drying is carried 40 product. out in vacuo in order to permit greater speed but We do not wish to limit the present invention the important thing is to ma the temperato any particular theory but we believe that the ture at a point below that at which the material wet mixing and subsequent drying of all the inis damaged and any drying method which permits gredients effects not only a more thorough admix maintaining a low t pe y be p y 45 ture but probably produces a chemical reaction Althoug t l m ted to a Particular p e, between certain of the constituents, notably the we prefer to use temperatures not exceeding 60 alkali and gum, altering their characteristics and to 65 C. producing a product which on the addition of The invention will be described in conjunction aqueous media readily rehydrates and forms a with the following specific examples which illustrate typical combinations of various colors with different proportions of paste forming ingredients. The invention is not limited to the details set forth in the specific examples which are intended to be typical illustrations only. More particularly, the procedure of drying, aging, etc.,

The above theory is advanced only as a probable explanation and it is possible that other factors are involved. Therefore, the invention is not limited to any theory.

55 The products of the present invention may be iven'in the examples is not intended to limit the invention as any of the other standard methods of drying, aging and the like may be used. The parts are by weight.

Example 1 A printing-thickener is prepared by heating 2000 parts of British Gum No. 1'77 (Stein Hall) and 6000 parts of cold water in a double boiler with continuous stirring at a temperature from 85 to 88 C. for 90 to 120 minutes. The source of heat is removed, the stirring continued, and 450 parts of potassium carbonate and 450 parts of sodium carbonate immediately added. When the thickener has cooled to approximately 66 C., 900 parts of sodium formaldehyde sulfoxylate are thoroughly incorporated. Subsequently, sufficient water is added to bring the total to 10,000 parts.

25 parts of a dispersible Vat Navy Blue powder (chlorinated dibenzanthrone) containing 32% real dyestufi and prepared according to United States Patent No. 2,090,511 are added to 975 parts of the above thickener and after thorough stirring, dried under 29 inches of vacuum in an aluminum pan at 60 to 65 C. for approximately 72 hours. After being dried, the product is crushed to yield coarse flakes.

These flakes are re-hydrated to give a printing color paste containing 36.6% solids which is essentially the same amount of real dye as is pres ent in the printing color paste before drying. The

- re-hydrated paste is slightly thicker than printing color pastes prepared in the usual manner from similar ingredients. It is reduced with water to the same apparent consistency as tested by hand-stirring, struck oil on bleached and mercerized square cotton cloth, dried in an oven at 60 to 80 C., aged for five minutes in a steam box at 104 C., soaped at'the boil with 0.5% soap solution, and then ironed dry. The resultant print is redder and stronger than that obtained from an ordinary printing paste of equivalent dye strength prepared from the same percentages of ingredients.

Example 2 25 parts of Vat Yellow GC powder (Color Index 1118) prepared according to United States Patent No. 2,090,511 are added to 975 parts of the thickening agent prepared as in Example 1 and the procedure of Example 1 followed, except the paste was dried in a copper tray.

63.4 parts of cold water are added to 36.6 parts of the solid material obtained as above described, forming a smooth printing paste which is further diluted with 5 parts of water to yield a product with satisfactory printing consistency. This color is printed, aged, oxidized, and finished as in Example 1 and the resulting print is redder and stronger than that obtained from an ordinary printing paste prepared from the same components.

Example 3 Using the procedure of Example 2, 25 parts of Vat Pink (6,6'-dichloro-4,4'-dimethyl-2,2'-bisthionaphthenindigo) powder, prepared according to United States Patent No. 2,090,511, are added to 9'75 parts of printing thickener as described in Example 1, and the mixture dried in a copper tray. The dried product is then coarsely ground to yield small pellets.

63.4 parts of water are added to 36.6 parts of these pellets yielding a paste. Prints made therefrom on cotton are yellower and appreciably stronger than those obtained from a portion of the same printing color paste which had not been dried, ground and rehydrated.

Example 4 25 parts of Orange R. powder, Color Index 1217, prepared according to United States Patent No. 2,090,511 and containing about 6 parts real dye, are added to 9'75 parts of the printing thickener prepared as in Example 1, intimately mixed and handled as in Example 2.

63.4 parts of cold water are added to 36.6 parts of this dried material and the mixture stirred until the paste is uniform. It is then printed on bleached, unmercerized 80 square cotton cloth, and finished in the usual manner. The resulting prints are yellower and their'color value is equal to the prints obtained from the original undried printing color paste, which had not been: dried, ground and rehydrated.

Example 5 A printing thickener is prepared by thoroughly mixing 2100 parts of B-2 British gum, 200 parts of tapioca flour, 500 parts of cornstarch and 2500 parts of cold water and heating in a double boiler with constant stirring until 1300 parts of water have evaporated, about to minutes. ring is continued until the paste has cooled.

400 parts of the above thickener are charged into a laboratory dough mixer, 100 parts of powdered potassium carbonate added thereto, and the mixture worked until uniform. parts of sulfoxylate, 60 parts of glycerine and 100 parts of Scarlet 2 GHN powder or a mixture of I-Lvdron Pink and Hydron Orange, containing about 36 parts of real dye, are added in the order given, each being intimately mixed before the addition of the next ingredient. The product is dried under 29 inches of vacuum in an aluminum pan at 60 to 65 C. This product puffs readily in the vacuum oven which is an asset in obtaining an easier rehydratable powder. The dried product is ground to give a fine powder, which, when rehydrated and printed, gives a smooth scarlet print of good color value.

Example 6 The procedure of Example 5 is followed exactly except that an additional one part of alpha anthraquinonyl-monamide of maleic acid is added as a printing assistant. The product is dried in an aluminum tray in vacuo and ground to a fine powder.

Example 7 gives a better color yield than Example 5 when rehydrated and printed on cotton.

Example 8 A sample of wet presscake of the dyestuff used in Example 2 is dispersed with the sodium salt of disulfodinaphthylmethane and adjusted with Water to contain 15% real color. 10 parts of this slurry is mixed with 90 parts of printing thickener prepared as in Example 1 except that 6% glycerine by weight is added prior to making up Stir- Example 9 The procedure of Example 5 is followed except that parts of the Vat Pink powder described in Example 3 is used as the dyestuff and the product is dried in vacuo at 60 to 65 C. When printed on pigmented rayon, a strong, b-right,,

pink print is obtained.

Example 10 The procedure of Example 9 is followed with the addition of 1% ferric chloride on the weight of the final powder, during the formulation. Prints from this material after rehydration give color yields much stronger than those obtained in Example 9.

Example 11 The procedure of Example 9 is followed except for the substitution of 1% aluminum sulfate for the ferric chloride. Prints after rehydration are superior to those obtained in Example 9.

Eaample 12 The procedure of Example 9 is followed with the substitution of beta methyl umbelliferon for the ferric chloride. Prints obtained from this product are superior to those obtained from the product prepared in Example 9.

Example 13 The procedure of Example 9 is followed with the addition of 60 parts of the butyl ether of ethyleneglycol with the glycerine. Prints obtained from this product are superior to those obtained from the product prepared in Example 9.

Example 14 The procedure of Example 13 is followed, substituting diethylene glycol for the butyl ether of ethyleneglycol. Prints obtained from this product are superior to those obtainedfrom the product prepared in Example 9.

Example 15 2100 parts of 3-2 British gum, 500 parts of cornstarch and 200 parts of tapioca flour are slurried with 1080 parts of Vat Pink presscake (Example 3), containing 300 parts real dye, dispersed with the sodium salt of 'disulfodinaphthylmethane, and 2200 parts of cold water. The mixture is cooked with stirring until the total weight is 4300. The heat is then removed, 1000 parts of solid potassium carbonate being added and the stirring continued until the solution is completed. When this mixture has cooled to approximately 65 C., 1600 parts of sulfoxylate are added and the stirring continued until dissolved, after which 600 parts of glycerine are added and the stirring is continued until the material is cooled down. This mix is dried at 60 to 65 C. in vacuo. The prints obtained'from the rehydrated product are bright and strong.

Example 16 A dispersed powder is prepared by treating 56 parts of an equimolar mixture of 2-methyl-5- chlorobenzene-diazo-blguanide and the orthotoluide of 2-hydroxy-3-carboxy naphthalene with ing thickening agent, until homogeneous admix- 3 parts of the sodium salt ofdisulfodinaphthylmethane, 70 parts water, 40 parts dextrine and 2 parts trisodium phosphate according to the method described in United States Patent No. 2,090,511. 20 parts of this powder are mixed with 56 parts of water, 24'parts of 5 N sodium hydroxide solution, 20 parts of Cellosolve and 80 parts of a neutralized starch-tragacanth paste, prepared by slurrying parts wheat starch in 850 parts water, adding 150 parts gum tragacanth (make up 6 oz. per gallon) then cooking in a double boiler, at to F. for 2 hours with stirring. After intimate mixing is accomplished, the material is vacuum dried for 12 hours at approximately 100 -F. then further dried for 6 hours at 160 F. When the product is re-hydrated, printed on a cellulose fabric and acid aged, it gives a print of excellent strength and brightness.

What we claim is:

1. A dispersible solid product capable of dis persion in aqueous media to give a finished printing paste comprising in combination a color, an alkali, and print thickening ingredients, the said components having been admixed in wet form and dried at a temperature below that at which the dehydration becomes irreversible.

2. A dispersible solid product capable of dispersion in aqueous media to give a finished printing paste comprising in combination a vat dye, an alkali, a reducing agent capable of transforming the vat dye into the leuco compound, and the printing thickening ingredients, the said components having been admixed in wet form and dried at a temperature below that at which the dehydration becomes irreversible.

3. A dispersible solid product capable of dispersion in aqueous media to give a finished printing paste comprising in combination a diazo compound stabilized against coupling in alkaline solution, a coupling component, an alkali and the printing thickening ingredients, the said components having been admixed in wet form and dried at a temperature below that at which the dehydration becomes irreversible.

4. A dispersible solid product capable of dispersion in aqueous media to give a finished printing paste comprising in combination a vat dye, an alkali, a reducing agent capable of transforming the vat dye into the leuco compound, printing thickening ingredients and a printing assistant, the said components having been admixed in wet form and dried at a temperature below that at which the dehydration becomes irreversible.

5. A dispersible solid product capable "of dispersion in aqueous media to give a finished printing paste comprising in combination a vat dye, an alkali, a reducing agent capable of transforming the vat dye into the leuco compound, printing thickening ingredients and a hygroscopicity modifying agent, the said components having been admixed in wet form and dried at a temperature below that at which the dehydration becomes irreversible.

6. A method of producing a solid product capable of forming a. printing paste on mixture with an aqueous medium which comprises mixing in aqueous dispersion a color, an alkali, and a printture results and drying the product at a temperature below that at which the dehydration becomes irreversible.

7. A method of producing a solid product capable of forming a printing paste on mixture with an aqueous medium which comprises mixing in aqueous dispersion a vat dye, an alkali, a reducing agent capable of transforming the vat dye into the lueco compound and printing thickening ingredients until homogeneous admixture results and drying the product at a temperature below that at which the dehydration becomes irreversible.

8. A method of producing a solid product capable of forming 2, pr iting paste on mixture with an aqueous medium which comprises mixing in aqueous dispersion a diazo compound stabilized against coupling in alkaline solution, a coupling component, an alkali, and printing thickening ingredients until homogeneous admixture results and drying the product at a temperature below that at which the dehydration becomes irreversible.

9. A method of producing a solid product capable of forming a printing paste on mixture with an aqueous medium which comprises mixing in aqueous dispersion, a vat dye, an alkali, a reducing agent capable of transforming the vat dye into the leuco compound, printing thickening inat a temperature below that at which the dehydration becomes irreversible.

10. A method of producing a solid product capable of forming a printing paste on mixture with an aqueous medium which comprises mixing in aqueous dispersion, a vat dye, an alkali, a reducing agent capable of transforming the vat dye mm the leuco compound, printing thickening ingredients and a hygroscopicity modifying agent until homogeneous admixture results and drying the product at a temperature below that at which the dehydration becomes irreversible.

11. A process according to claim 7 in which all of the components are mixed in the form of a stiff aqueous paste.

12. A process according to claim 8 in which all of the components are mixed in the form of a stiff aqueous paste.

MOSES L. CROSSIE'Y. ROY H. KIENLE. CHES'I'ER A. AMICK. 

